傅立叶变换衰减全反射红外光谱法测定药用卤化丁基橡胶塞表面残留硅油量

目的: 建立傅立叶变换衰减全反射红外光谱(FTIR-ATR)法测定药用卤化丁基橡胶塞表面硅油量。 方法: 样品经乙醚回流提取,溶剂挥干后,用三氯甲烷溶解并定容,直接加样至傅立叶变换红外光谱仪的ZnSe晶体样品槽,扫描红外谱图。利用二甲基硅油在(1260±10)cm^-1波数的特征吸收峰峰面积定量测定。 结果: 二甲基硅油在1.2~32.1 mg·mL^-1范围内呈良好的线性关系,r=0.9983。二甲基硅油的LOQ为1.2 mg·mL^-1,平均回收率为92.1%。 结论: 本方法灵敏,准确可靠,可用于药用卤化丁基橡胶塞表面残留硅油的定量测定。

Objective: To establish a fourier transform infrared spectroscopy-attenuated total reflection spectra (FTIR-ATR)method for determination of polydimethylsiloxane on the surface of butyl rubber stoppers. Methods: The butyl rubber stoppers were circum-fluence extracted by ether.The extraction was dissolved and diluted to definite volume by methenyl chloride after vaporizing the solvent absolutely.The specific absorption peak of polydimethylsioxane at (1260±10)cm^-1 was used as detecting peaks. Results: The linear range of polydimethylsiloxane was about 1.2-32.1 mg·mL^-1 and its correlation coefficient was 0.9983.The average recovery of the method was 92.1%.The LOQ of polydimethylsiloxane was 1.2 mg·mL^-1. Conclusion: The method is simple,accurate and can be used to determine residual polydimethylsiloxane on the surface of butyl rubber stoppers.